# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kenneth Caulton' _publ_contact_author_email CAULTON@INDIANA.EDU _publ_section_title ; Unusual Selectivity of a (pincer)Ni-hydride Reacting with CO2 ; loop_ _publ_author_name 'Kenneth Caulton' 'Hongjun Fan' 'Matthew F Laird' 'Maren Pink' 'Nikolay P Tsvetkov' # Attachment '08091.cif' data_08091 _database_code_depnum_ccdc_archive 'CCDC 698861' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H53 N Ni O2 P2 Si2' _chemical_formula_sum 'C23 H53 N Ni O2 P2 Si2' _chemical_formula_weight 552.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.9617(7) _cell_length_b 9.9816(4) _cell_length_c 17.4523(7) _cell_angle_alpha 90.00 _cell_angle_beta 106.4510(10) _cell_angle_gamma 90.00 _cell_volume 3000.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9978 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.223 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.852 _exptl_absorpt_correction_type multi-scans _exptl_absorpt_correction_T_min 0.8414 _exptl_absorpt_correction_T_max 0.8973 _exptl_absorpt_process_details 'SADABS, R. Blessing; 1995' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_details '0.30 degree frames measured for 30 seconds each' _diffrn_measurement_method 'omega and phi scans' _diffrn_measurement_device 'APEX Kappa Duo' _diffrn_measurement_device_type Kappa _diffrn_detector 'CCD area detector' _diffrn_detector_type 'Bruker APEXII' _diffrn_detector_area_resol_mean 83.33 _diffrn_reflns_number 26119 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_sigmaI/netI 0.0218 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.18 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6895 _reflns_number_gt 6169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX II v.2.2 (Bruker, 2007)' _computing_cell_refinement 'APEX II v.2.2 (Bruker, 2007)' _computing_data_reduction 'APEX II v.2.2 (Bruker, 2007)' _computing_structure_solution 'SIR-2004 (Burla et al., 2005)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Bruker, 2008)' _computing_publication_material 'SHELXTL (Bruker, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+1.1227P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6895 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0291 _refine_ls_R_factor_gt 0.0243 _refine_ls_wR_factor_ref 0.0671 _refine_ls_wR_factor_gt 0.0641 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni1 Ni 0.787453(10) 0.020632(16) 0.884012(10) 0.01806(5) Uani 1 1 d . . . H1NI H 0.7682 -0.0963 0.9138 0.037(5) Uiso 1 1 d R . . P1 P 0.707672(19) 0.10208(3) 0.948127(19) 0.01701(7) Uani 1 1 d . . . P2 P 0.840688(19) -0.14544(3) 0.83377(2) 0.01826(8) Uani 1 1 d . . . Si1 Si 0.61437(2) -0.19293(4) 0.92855(2) 0.01952(8) Uani 1 1 d . . . Si2 Si 0.66373(2) -0.24239(4) 0.77081(2) 0.01896(8) Uani 1 1 d . . . N1 N 0.82316(8) 0.17920(12) 0.84610(8) 0.0299(3) Uani 1 1 d . . . O1 O 0.65155(6) -0.24887(10) 0.85996(6) 0.0246(2) Uani 1 1 d . . . O2 O 0.85994(10) 0.37993(13) 0.79399(8) 0.0608(4) Uani 1 1 d . . . C1 C 0.50760(9) -0.22286(17) 0.89567(11) 0.0354(4) Uani 1 1 d . . . H1A H 0.4975 -0.3191 0.8876 0.053 Uiso 1 1 calc R . . H1B H 0.4846 -0.1752 0.8454 0.053 Uiso 1 1 calc R . . H1C H 0.4845 -0.1900 0.9367 0.053 Uiso 1 1 calc R . . C2 C 0.65622(10) -0.29418(15) 1.01968(9) 0.0310(3) Uani 1 1 d . . . H2A H 0.6407 -0.3880 1.0090 0.046 Uiso 1 1 calc R . . H2B H 0.6371 -0.2604 1.0633 0.046 Uiso 1 1 calc R . . H2C H 0.7130 -0.2876 1.0349 0.046 Uiso 1 1 calc R . . C3 C 0.62255(8) -0.00523(13) 0.94267(8) 0.0206(3) Uani 1 1 d . . . H3A H 0.5800 0.0327 0.8989 0.025 Uiso 1 1 calc R . . H3B H 0.6084 0.0127 0.9926 0.025 Uiso 1 1 calc R . . C4 C 0.75907(8) 0.12035(13) 1.05778(8) 0.0214(3) Uani 1 1 d . . . C5 C 0.71448(9) 0.19832(16) 1.10649(9) 0.0284(3) Uani 1 1 d . . . H5A H 0.7425 0.1927 1.1634 0.043 Uiso 1 1 calc R . . H5B H 0.6625 0.1597 1.0974 0.043 Uiso 1 1 calc R . . H5C H 0.7099 0.2924 1.0897 0.043 Uiso 1 1 calc R . . C6 C 0.83824(8) 0.18701(15) 1.06663(9) 0.0274(3) Uani 1 1 d . . . H6A H 0.8675 0.1905 1.1233 0.041 Uiso 1 1 calc R . . H6B H 0.8303 0.2782 1.0450 0.041 Uiso 1 1 calc R . . H6C H 0.8674 0.1348 1.0372 0.041 Uiso 1 1 calc R . . C7 C 0.77463(9) -0.02072(15) 1.09357(9) 0.0283(3) Uani 1 1 d . . . H7A H 0.8069 -0.0145 1.1491 0.042 Uiso 1 1 calc R . . H7B H 0.8017 -0.0739 1.0625 0.042 Uiso 1 1 calc R . . H7C H 0.7252 -0.0639 1.0920 0.042 Uiso 1 1 calc R . . C8 C 0.65808(8) 0.26655(13) 0.90861(8) 0.0223(3) Uani 1 1 d . . . C9 C 0.62953(9) 0.25146(14) 0.81707(9) 0.0282(3) Uani 1 1 d . . . H9A H 0.6028 0.3336 0.7935 0.042 Uiso 1 1 calc R . . H9B H 0.5936 0.1756 0.8033 0.042 Uiso 1 1 calc R . . H9C H 0.6740 0.2356 0.7962 0.042 Uiso 1 1 calc R . . C10 C 0.58708(9) 0.30252(15) 0.93755(10) 0.0291(3) Uani 1 1 d . . . H10A H 0.5640 0.3861 0.9121 0.044 Uiso 1 1 calc R . . H10B H 0.6034 0.3141 0.9957 0.044 Uiso 1 1 calc R . . H10C H 0.5487 0.2303 0.9232 0.044 Uiso 1 1 calc R . . C11 C 0.71573(9) 0.38372(14) 0.92834(10) 0.0280(3) Uani 1 1 d . . . H11A H 0.6922 0.4630 0.8979 0.042 Uiso 1 1 calc R . . H11B H 0.7630 0.3596 0.9140 0.042 Uiso 1 1 calc R . . H11C H 0.7289 0.4034 0.9856 0.042 Uiso 1 1 calc R . . C12 C 0.60851(9) -0.38606(15) 0.71324(9) 0.0271(3) Uani 1 1 d . . . H12A H 0.5557 -0.3867 0.7188 0.041 Uiso 1 1 calc R . . H12B H 0.6346 -0.4702 0.7340 0.041 Uiso 1 1 calc R . . H12C H 0.6062 -0.3767 0.6567 0.041 Uiso 1 1 calc R . . C13 C 0.62587(9) -0.08125(15) 0.72206(9) 0.0297(3) Uani 1 1 d . . . H13A H 0.6580 -0.0074 0.7505 0.045 Uiso 1 1 calc R . . H13B H 0.5722 -0.0687 0.7236 0.045 Uiso 1 1 calc R . . H13C H 0.6274 -0.0826 0.6664 0.045 Uiso 1 1 calc R . . C14 C 0.76788(8) -0.26413(13) 0.77454(8) 0.0217(3) Uani 1 1 d . . . H14A H 0.7837 -0.3553 0.7952 0.026 Uiso 1 1 calc R . . H14B H 0.7712 -0.2613 0.7189 0.026 Uiso 1 1 calc R . . C15 C 0.90415(8) -0.25160(13) 0.91689(9) 0.0228(3) Uani 1 1 d . . . C16 C 0.95123(9) -0.15661(16) 0.98186(10) 0.0321(3) Uani 1 1 d . . . H16A H 0.9832 -0.2092 1.0266 0.048 Uiso 1 1 calc R . . H16B H 0.9157 -0.0996 1.0008 0.048 Uiso 1 1 calc R . . H16C H 0.9848 -0.1004 0.9597 0.048 Uiso 1 1 calc R . . C17 C 0.85128(9) -0.33693(15) 0.95313(10) 0.0309(3) Uani 1 1 d . . . H17A H 0.8825 -0.3790 1.0025 0.046 Uiso 1 1 calc R . . H17B H 0.8261 -0.4065 0.9150 0.046 Uiso 1 1 calc R . . H17C H 0.8116 -0.2796 0.9650 0.046 Uiso 1 1 calc R . . C18 C 0.95948(9) -0.34689(15) 0.89108(10) 0.0314(3) Uani 1 1 d . . . H18A H 0.9865 -0.4032 0.9364 0.047 Uiso 1 1 calc R . . H18B H 0.9975 -0.2946 0.8730 0.047 Uiso 1 1 calc R . . H18C H 0.9298 -0.4038 0.8473 0.047 Uiso 1 1 calc R . . C19 C 0.89448(8) -0.09494(14) 0.75934(9) 0.0250(3) Uani 1 1 d . . . C20 C 0.96497(9) -0.00888(15) 0.80156(11) 0.0328(3) Uani 1 1 d . . . H20A H 0.9886 0.0277 0.7619 0.049 Uiso 1 1 calc R . . H20B H 1.0030 -0.0642 0.8398 0.049 Uiso 1 1 calc R . . H20C H 0.9482 0.0648 0.8299 0.049 Uiso 1 1 calc R . . C21 C 0.92187(11) -0.21078(16) 0.71579(11) 0.0374(4) Uani 1 1 d . . . H21A H 0.9401 -0.1748 0.6721 0.056 Uiso 1 1 calc R . . H21B H 0.8786 -0.2725 0.6941 0.056 Uiso 1 1 calc R . . H21C H 0.9644 -0.2588 0.7535 0.056 Uiso 1 1 calc R . . C22 C 0.83713(10) -0.01029(16) 0.69579(9) 0.0327(3) Uani 1 1 d . . . H22A H 0.8639 0.0280 0.6591 0.049 Uiso 1 1 calc R . . H22B H 0.8167 0.0621 0.7219 0.049 Uiso 1 1 calc R . . H22C H 0.7942 -0.0670 0.6658 0.049 Uiso 1 1 calc R . . C23 C 0.84168(10) 0.27744(15) 0.82088(9) 0.0323(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.01912(9) 0.01473(9) 0.02098(9) -0.00159(6) 0.00674(7) -0.00101(6) P1 0.01699(16) 0.01472(15) 0.01860(16) -0.00041(12) 0.00388(13) 0.00021(12) P2 0.01801(16) 0.01518(15) 0.02263(17) -0.00267(12) 0.00747(13) -0.00230(12) Si1 0.02111(18) 0.01962(18) 0.01895(17) -0.00024(13) 0.00749(14) -0.00296(13) Si2 0.01991(18) 0.01935(17) 0.01738(17) -0.00227(13) 0.00491(14) -0.00312(13) N1 0.0391(7) 0.0191(6) 0.0376(7) -0.0009(5) 0.0209(6) -0.0011(5) O1 0.0278(5) 0.0265(5) 0.0214(5) -0.0034(4) 0.0104(4) -0.0056(4) O2 0.0955(12) 0.0375(7) 0.0460(8) 0.0068(6) 0.0145(8) -0.0322(7) C1 0.0252(8) 0.0356(8) 0.0470(10) -0.0042(7) 0.0128(7) -0.0087(6) C2 0.0488(10) 0.0226(7) 0.0235(7) 0.0017(6) 0.0134(7) 0.0001(6) C3 0.0180(6) 0.0203(6) 0.0230(7) 0.0006(5) 0.0051(5) -0.0004(5) C4 0.0201(6) 0.0229(7) 0.0199(6) -0.0021(5) 0.0034(5) 0.0011(5) C5 0.0253(7) 0.0357(8) 0.0238(7) -0.0061(6) 0.0060(6) 0.0027(6) C6 0.0192(7) 0.0305(7) 0.0296(7) -0.0052(6) 0.0021(6) -0.0019(6) C7 0.0327(8) 0.0271(7) 0.0225(7) 0.0027(6) 0.0034(6) 0.0027(6) C8 0.0228(7) 0.0166(6) 0.0258(7) 0.0010(5) 0.0040(5) 0.0029(5) C9 0.0335(8) 0.0218(7) 0.0253(7) 0.0049(5) 0.0020(6) 0.0035(6) C10 0.0250(7) 0.0246(7) 0.0367(8) 0.0004(6) 0.0070(6) 0.0070(6) C11 0.0320(8) 0.0157(6) 0.0367(8) -0.0007(6) 0.0107(7) -0.0003(5) C12 0.0275(7) 0.0279(7) 0.0246(7) -0.0048(6) 0.0054(6) -0.0083(6) C13 0.0362(8) 0.0262(7) 0.0251(7) -0.0014(6) 0.0061(6) 0.0045(6) C14 0.0224(7) 0.0206(6) 0.0224(6) -0.0060(5) 0.0069(5) -0.0038(5) C15 0.0210(7) 0.0186(6) 0.0270(7) -0.0006(5) 0.0042(6) -0.0005(5) C16 0.0276(8) 0.0300(8) 0.0334(8) -0.0074(6) 0.0001(6) -0.0012(6) C17 0.0324(8) 0.0255(7) 0.0342(8) 0.0066(6) 0.0087(7) -0.0006(6) C18 0.0269(8) 0.0229(7) 0.0427(9) -0.0023(6) 0.0070(7) 0.0049(6) C19 0.0296(7) 0.0193(6) 0.0313(7) -0.0017(5) 0.0173(6) -0.0032(5) C20 0.0284(8) 0.0263(7) 0.0489(10) -0.0011(7) 0.0190(7) -0.0072(6) C21 0.0470(10) 0.0280(8) 0.0484(10) -0.0069(7) 0.0316(8) -0.0028(7) C22 0.0454(10) 0.0299(8) 0.0263(8) 0.0007(6) 0.0158(7) -0.0010(7) C23 0.0432(9) 0.0256(8) 0.0277(7) -0.0037(6) 0.0097(7) -0.0091(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ni1 N1 1.8959(12) . ? Ni1 P1 2.2079(4) . ? Ni1 P2 2.2149(4) . ? Ni1 H1NI 1.3612 . ? P1 C3 1.8470(14) . ? P1 C4 1.8833(14) . ? P1 C8 1.9017(14) . ? P2 C14 1.8485(13) . ? P2 C19 1.8938(14) . ? P2 C15 1.8947(14) . ? Si1 O1 1.6258(10) . ? Si1 C2 1.8545(15) . ? Si1 C1 1.8637(16) . ? Si1 C3 1.8900(14) . ? Si2 O1 1.6326(10) . ? Si2 C13 1.8563(15) . ? Si2 C14 1.8659(14) . ? Si2 C12 1.8669(14) . ? N1 C23 1.161(2) . ? O2 C23 1.2090(19) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C7 1.5336(19) . ? C4 C5 1.5349(18) . ? C4 C6 1.5376(19) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C11 1.5351(19) . ? C8 C9 1.541(2) . ? C8 C10 1.5412(19) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.5326(19) . ? C15 C16 1.535(2) . ? C15 C17 1.539(2) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.535(2) . ? C19 C22 1.536(2) . ? C19 C21 1.539(2) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Ni1 P1 101.64(4) . . ? N1 Ni1 P2 105.07(4) . . ? P1 Ni1 P2 153.014(14) . . ? N1 Ni1 H1NI 175.2 . . ? P1 Ni1 H1NI 81.4 . . ? P2 Ni1 H1NI 72.2 . . ? C3 P1 C4 105.60(6) . . ? C3 P1 C8 100.72(6) . . ? C4 P1 C8 109.23(6) . . ? C3 P1 Ni1 114.01(4) . . ? C4 P1 Ni1 110.42(4) . . ? C8 P1 Ni1 116.02(5) . . ? C14 P2 C19 101.80(6) . . ? C14 P2 C15 104.28(6) . . ? C19 P2 C15 111.16(6) . . ? C14 P2 Ni1 112.62(4) . . ? C19 P2 Ni1 115.70(4) . . ? C15 P2 Ni1 110.43(4) . . ? O1 Si1 C2 107.04(6) . . ? O1 Si1 C1 108.65(7) . . ? C2 Si1 C1 107.97(8) . . ? O1 Si1 C3 113.80(6) . . ? C2 Si1 C3 115.51(7) . . ? C1 Si1 C3 103.55(7) . . ? O1 Si2 C13 109.91(6) . . ? O1 Si2 C14 111.45(6) . . ? C13 Si2 C14 110.50(7) . . ? O1 Si2 C12 106.76(6) . . ? C13 Si2 C12 110.43(7) . . ? C14 Si2 C12 107.70(6) . . ? C23 N1 Ni1 176.97(15) . . ? Si1 O1 Si2 151.87(7) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? P1 C3 Si1 127.90(7) . . ? P1 C3 H3A 105.3 . . ? Si1 C3 H3A 105.3 . . ? P1 C3 H3B 105.3 . . ? Si1 C3 H3B 105.3 . . ? H3A C3 H3B 106.0 . . ? C7 C4 C5 107.66(12) . . ? C7 C4 C6 107.44(12) . . ? C5 C4 C6 109.74(12) . . ? C7 C4 P1 107.77(9) . . ? C5 C4 P1 115.43(10) . . ? C6 C4 P1 108.50(9) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C4 C7 H7A 109.5 . . ? C4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C11 C8 C9 108.20(12) . . ? C11 C8 C10 108.49(11) . . ? C9 C8 C10 107.41(12) . . ? C11 C8 P1 111.07(10) . . ? C9 C8 P1 106.01(9) . . ? C10 C8 P1 115.36(10) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P2 C14 Si2 119.24(7) . . ? P2 C14 H14A 107.5 . . ? Si2 C14 H14A 107.5 . . ? P2 C14 H14B 107.5 . . ? Si2 C14 H14B 107.5 . . ? H14A C14 H14B 107.0 . . ? C18 C15 C16 109.45(12) . . ? C18 C15 C17 107.72(12) . . ? C16 C15 C17 108.27(12) . . ? C18 C15 P2 114.94(10) . . ? C16 C15 P2 107.82(10) . . ? C17 C15 P2 108.47(10) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C22 109.41(12) . . ? C20 C19 C21 108.79(12) . . ? C22 C19 C21 107.44(13) . . ? C20 C19 P2 109.35(10) . . ? C22 C19 P2 105.88(10) . . ? C21 C19 P2 115.81(10) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C23 O2 179.1(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Ni1 P1 C3 145.91(7) . . . . ? P2 Ni1 P1 C3 -25.79(6) . . . . ? N1 Ni1 P1 C4 -95.40(6) . . . . ? P2 Ni1 P1 C4 92.89(6) . . . . ? N1 Ni1 P1 C8 29.54(7) . . . . ? P2 Ni1 P1 C8 -142.16(5) . . . . ? N1 Ni1 P2 C14 -123.78(7) . . . . ? P1 Ni1 P2 C14 47.81(6) . . . . ? N1 Ni1 P2 C19 -7.26(7) . . . . ? P1 Ni1 P2 C19 164.33(6) . . . . ? N1 Ni1 P2 C15 120.09(6) . . . . ? P1 Ni1 P2 C15 -68.32(6) . . . . ? C2 Si1 O1 Si2 -175.32(14) . . . . ? C1 Si1 O1 Si2 68.32(16) . . . . ? C3 Si1 O1 Si2 -46.46(16) . . . . ? C13 Si2 O1 Si1 11.81(16) . . . . ? C14 Si2 O1 Si1 134.67(14) . . . . ? C12 Si2 O1 Si1 -107.98(15) . . . . ? C4 P1 C3 Si1 -94.60(10) . . . . ? C8 P1 C3 Si1 151.76(9) . . . . ? Ni1 P1 C3 Si1 26.80(11) . . . . ? O1 Si1 C3 P1 -44.24(11) . . . . ? C2 Si1 C3 P1 80.19(11) . . . . ? C1 Si1 C3 P1 -161.99(10) . . . . ? C3 P1 C4 C7 53.86(11) . . . . ? C8 P1 C4 C7 161.44(9) . . . . ? Ni1 P1 C4 C7 -69.83(10) . . . . ? C3 P1 C4 C5 -66.48(12) . . . . ? C8 P1 C4 C5 41.10(12) . . . . ? Ni1 P1 C4 C5 169.82(9) . . . . ? C3 P1 C4 C6 169.92(9) . . . . ? C8 P1 C4 C6 -82.51(10) . . . . ? Ni1 P1 C4 C6 46.22(10) . . . . ? C3 P1 C8 C11 164.24(10) . . . . ? C4 P1 C8 C11 53.39(11) . . . . ? Ni1 P1 C8 C11 -72.16(10) . . . . ? C3 P1 C8 C9 -78.45(10) . . . . ? C4 P1 C8 C9 170.69(9) . . . . ? Ni1 P1 C8 C9 45.14(10) . . . . ? C3 P1 C8 C10 40.27(12) . . . . ? C4 P1 C8 C10 -70.58(12) . . . . ? Ni1 P1 C8 C10 163.86(9) . . . . ? C19 P2 C14 Si2 -129.78(8) . . . . ? C15 P2 C14 Si2 114.53(8) . . . . ? Ni1 P2 C14 Si2 -5.23(10) . . . . ? O1 Si2 C14 P2 -58.71(10) . . . . ? C13 Si2 C14 P2 63.80(10) . . . . ? C12 Si2 C14 P2 -175.50(8) . . . . ? C14 P2 C15 C18 73.39(11) . . . . ? C19 P2 C15 C18 -35.56(12) . . . . ? Ni1 P2 C15 C18 -165.38(9) . . . . ? C14 P2 C15 C16 -164.25(10) . . . . ? C19 P2 C15 C16 86.80(11) . . . . ? Ni1 P2 C15 C16 -43.02(10) . . . . ? C14 P2 C15 C17 -47.22(11) . . . . ? C19 P2 C15 C17 -156.17(10) . . . . ? Ni1 P2 C15 C17 74.01(10) . . . . ? C14 P2 C19 C20 -172.80(10) . . . . ? C15 P2 C19 C20 -62.25(11) . . . . ? Ni1 P2 C19 C20 64.74(11) . . . . ? C14 P2 C19 C22 69.42(10) . . . . ? C15 P2 C19 C22 179.97(9) . . . . ? Ni1 P2 C19 C22 -53.04(11) . . . . ? C14 P2 C19 C21 -49.50(13) . . . . ? C15 P2 C19 C21 61.05(14) . . . . ? Ni1 P2 C19 C21 -171.96(11) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.458 _refine_diff_density_min -0.228 _refine_diff_density_rms 0.049